Potassium Carbonate → HCID 86689169, Verbindung

Temperatur

0 °C

To a solution of 5,6-dichloro-pyridin-3-ol [11860-92-9] (500 mg, 3.05 mmol) and K2CO3 (632 mg, 4.57 mmol) in dry ACN (12 ml) was added fluoro-iodomethane (1.156 ml, 9.15 mmol) at 0° C. The light yellow suspension was stirred for 5 min at 0° C. and then heated up to 120° C. for 30 min. Saturated aq. NH4Cl was added, followed by EtOAc. The organic layer was separated and the aqueous layer was extracted twice with EtOAc. The combined organic layers were washed with brine, dried with Na2SO4, filtered and evaporated to give a brown oil. The crude material was directly used in the next step without further purification.

1. temperatureheated up to 120° C. for 30 min
2. customThe organic layer was separated
3. extractionthe aqueous layer was extracted twice with EtOAc
4. washThe combined organic layers were washed with brine
5. dry with materialdried with Na2SO4
6. filtrationfiltered
7. customevaporated
8. customto give a brown oil
9. customThe crude material was directly used in the next step without further purification

ORD-Eintrag

ord-5d3803863bda469dac70d93e221b8515

Quelldatensatz

uspto-grants-2015_10

DOI

10.6084/m9.figshare.5104873.v1

Patentnummer

US09163011B2